Process of electrically preparing catalysts for hydrogenation.



i'rEn s'rarns rArEIN'r orricn.

CARLETON ELLIS, F MONTCLAIR, NEW JERSEY.

PROCESS OF ELECTRICALLY rnnramire CATALYSTS FOR HYDROGENATION.

No Drawing.-

To all whom it may concern.

Be it known that I, CARLETON ELLIS, a citizen of the United States, and a resident of Montclair, in. the county 'offEssex and State of New Jersey, ha e invented certain new and useful Improvements in Processes of Electrically Preparing Catalysts for Hydrogenation, of which .the following is a specification. This invention relates to the preparation of catalyzers adapted for use in the hydrogenation or hardening of fatty oils or similar material and relates particularly to the elec trolytic production of a catalyZen onipriS- mg active nickel and the like derived by electrical comminution 0): formation as by electrolytically depositing the metal as for example from a saline solution.

This invention contains mattendisclosed in my copending application Serial No. 686,988 filed Mar. 29, 1912. (From Serial No. 679,771). i

The object of the present invention is to "obtain a catalyzer by forming catalytic nickel by an electrical method so as to secure the metal in such an extended condition as to afford a very extensive surface for the action of hydrogen thereby enabling fatty oils containing unsaturated bodies such as olein.

to be saturated with hydrogen forming harder products of greater commercialvalue.

One embodiment of the present invention comprises the deposition of a metal such as nickel by electrolysis, as from asaline electrolyte, on a carrier or support Which'preferablyhas'an affinity or absorpti e capacity for hydrogen so that hydrogen may be 0':-

cluded by the mass of supporting material thereby forming a storehouse of the gas for the active or more active surfaces. Such cooperating supporting material may be, for example, charcoal, graphite or other suitable form 'of car'bon or it may be-a metal such as nickel in a form which may be inactive or only slightly active as regards the property of transmitting hydrogen to oil or nickel;

forming a hydrogen occluding support for. the more active nickel material. The lattei'q;

for example, maybe in the form of a metallic sponge coated on charcoal particles, powdered graphite or a metallic support. In order to deposit nickel from solution in this manner preferably a current of relatively' high density is employed. An electrolyte containing: nickel sulfate. or nickel ammonium sulfate may be employed, of prefer- Specification of Letters Patent.

:form of nickel. and some tltanlum material may likewise be Patent ed Apr. 8,1919.

' Application fi1ed=November 14, 1916. Serial No. 131,253.

" ably fairly weak concentration and to the mass there may be added a small amount about five per cent. or so of titanium salt. A nickel anode may be employed and the cathode may be a mass of powdered charcoal or graphite which is kept in motion during the deposition or the cathode may be of any other suitable material or support. A small amount of copper is sometimes desirable and this may be introduced into the electrolyte or otherwise. A small amount'of zinc sulfate enables the production of a. more spongy A mixed deposit of nickel obtainedwhichis eflicient as a catalyzer. The

titan-ium aids in modifying the character of the nickel so as to produce a greater measure of hydrogen absorption.

If any undesirable oxidation of the particles of catalytic material has occurred, these may be reduced exposing to a current of hydrogen at say 350" C., or they may bereduced in oil by passage of a current of hydrogen therethrough at 250 to 275 C. In the latter case the presence of a small amount of copper or titanium apparently' aids in the reduction or serves as an assistant -1n reduction. The material so prepared may be 1ntroduced 1nto fatty o1l heated to about 180 C. Hydrogen or a hydrogen containing gas is introduced and the oil hardened to a point. The electrolytically-deposited catalyzer may be placed in a towergthrough which the oil is caused to flow with hydrogen is effected and the hardened oil drawn off at the bottom of the towerin a continuous manner. Or the catalyzer'may be agitated with the oil inthepresenceof hydrogen to produce a hardened product.

The advantages of the electro'lyticnickel lyti-cally deposited nickel. is particularly suited as a source of catalytic material. By electrolysis under well regulategl conditions,

productof the desired melting while contact a very pure deposit of the metal is obtained. This often is diflicult by wet methods involving washing of precipitates. By way of illustration it may be noted that nickel from sulfates.

sulfate solution treated with alkali forms a precipitate which is very diflicult to free If this precipitate with or without a carrier is not completely freed of sulfates by tedious Washing and other special treatment sulfids may form on reduction with hydrogen at 350 or higher and the catalyzer will be poisoned. By the present method catalyzer is obtained without this serious contamination with sulfur so that an electrolyte such as nickel sulfate or nickel ammonium sulfate solution may be employed yielding eflicient catalytic material cheaply.

When the catalytic material is carried on a support which is porous and the latter becomes impregnated with the material it is even more diflicult to remove the occluding sulfate or basic sulfate which forms and. the reduction of the latter to form sulfids when the raw catalytic material is exposed" at high temperatures to a reducing gas yields a product which usually has very poor catalytic properties in fact so as to be incapable of use but once or twice and there-.

fore being practically inoperative in comparison with catalyzers which are so free from poisons that they may be used daily for weeks or months without serious impairment of their catalytic properties.

The advantages of electrical formation of nickel catalyzer also embrace the point that the metal may be deposited in a finely extended condition without resorting to reduction by means of hydrogen at high temperatures with undesirable sintering of the product and consequent loss in catalytic value. When nickel hydrate or other material is subjected to an atmosphere of hydro: gen but not in contact with oil or other liquid vehicle, ordinarily it is considered necessary to heat the finely divided material in such hy "lrogen atmosphere to a temperature of 40b to 500 C., and in some cases the catalyzer is" prepared at a fairly strong red heat. This tends to cause sintering and agglomeration of the particles and in consequence the surface exposure is not suflicient. In other words, the material shrinks or compacts to form a product having too little superficial area to effectually yield the requisite catalytic properties for the purpose in hand. The extension of the "catalyzer on a bulky carrier is a makeshift in the efiort to set forth it is primarily my object as statedin Serial No. 686,988, to produce a metallic sponge in a highly comminuted state and for thepurpose of producing such a metallic sponge of nickel or similar metal in a state of extreme comminution, I-preferably employ density so readily and suitably yielded in this condition.

To recapitulate the process of the present invention involves minuted state by electrical action.

The use of the catalyst prepared in accordance with the present invention isnot claimed herein, but in my co-pendingapplication, 118,750. What I claim is: 1. The process of forming finely-divided spongy nickel by electrical action which comprises passing an electric current of high density from a nickel electrode to a mass of charcoal material, both the nickel electrode and charcoal material being immersed m a liquid electrolyte; wherebymetallic sponge a current of relatively high' that the nickel, material w1ll be the forming of a metal sponge, preferably of nickel, in a highly comin a highly comminuted-state adapted for use as a hydrogenatmg catalyst isdeposited on said charcoal material. r

2. The process of producing a catalyst comprising finely-divided spongy nickel on a carbon base, byv electrical action, such process including the passage of an electric current of high density from to a mass of carbon, both the nickel elec-' trode and carbon being immersed in a liquid electrolyte; whereby porous spongy nickel adapted for use as a hydrogenatingcatalyst is deposited on said carbon; introducing the so-produced nickel-carbon catalyst into an organlc material containing unsaturated mater'lal and capable of. actmg as a sealing fluid.

CABLETON ELLIS.

a nickel electrode 

